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PL
Pięć konserwantów i słodzików (kwas sorbowy, PhCOOH, kwas dehydrooctowy, acesulfam K i sacharynian sodu) dodano do żywności (chleb, żółta brzoskwinia, kiełbasa z szynki), ekstrahowano wodą (stężenie 0-160 mg/L) i z powodzeniem analizowano na obecność dodatków za pomocą wysokosprawnej chromatografii cieczowej (faza ruchoma MeOH, rozpuszczalnik AcONH₄) przy szybkości przepływu 1,0 mL/min i długości fali detekcji 230 nm.
EN
Five preservatives and sweeteners (sorbic acid, PhCOOH, dehydroacetic acid, acesulfame K and saccharin Na) were added to foods (bread, yellow peach, ham sausage), extd. with water (concn. 0-160 mg/L) and analyzed successfully by high-performance liq. chromatog. (mobile phase MeOH soln. of AcONH₄) atflow rate 1.0 mL/min and detection wavelength 230 nm for presence of additives.
EN
In this study, we propose a simple, cost-effective, and sensitive high-performance liquid chromatography with both detection techniques such as diode-array detection and fluorescence detection (HPLC-DAD-FLD) for the determination of nesfatin-1 in fetal bovine serum samples. The limit of detection (LOD) and limit of quantification (LOQ) for nesfatin-1 were set at satisfactory values in the range 0.22–0.35 mg mL⁻¹ and in the range 0.67–1.05 mg mL⁻¹, respectively (at two different wavelengths (DAD) and at four different wavelengths (FLD)). Analyte concentrations were determined as the average value from fetal bovine serum matrix samples. The preliminary results show that the SPE procedure on Isolute Si-TsOH (SCX-3) could be used for further nesfatin-1 analyses in human serum samples. Both the SPE technique, chromatographic analysis with gradient elution mode and detection technique are fast and convenient.
EN
Phytoplankton composition, abundance and carbon biomass were investigated at monthly intervals during 2006–2007 at a coastal site, “Acqua Alta” an oceanographic tower, in the northern Adriatic Sea. Results were compared with chlorophyll a concentrations of phytoplankton classes attributed by HPLC-CHEMTAX analysis. Changes in the taxonomic structure were associated with environmental parameters. The total carbon biomass of phytoplankton was positively correlated with the temperature and negatively correlated with silicate concentrations. Nutrient concentrations were higher in the winter–spring period than in the summer-autumn period. The highest carbon biomass and abundance of phytoplankton were observed during summer–autumn months. Diatoms were the group that had the highest contribution to the total carbon biomass during the sampling period. Small flagellates, which were the major contributors to the total cell counts were dominant during the summer period. There was a significant correlation between carbon biomass and CHEMTAX-derived Chl a values of diatoms and dinoflagellates. However, the total carbon biomass of phytoplankton was not correlated with Chl a, which seemed to be related to seasonal changes in the ratios of C:Chl a of all taxonomic classes. This ratio was higher during the summer-autumn period (73 ± 33) than during the winter–spring period (17 ± 20).
4
Content available remote Quick Detection of Aldehydes and Ketones in Automotive Textiles
EN
This study was aimed to develop a quick detection method to test aldehydes and ketones in textiles in order to control the quality of automotive textiles in the development process from fabric production to end-use in vehicles. In this study, a pretreatment of samples was applied to simulate the actual environment of textiles used in vehicles. Collected volatiles were reacted with 2,4-dinitrophenylhydrazine and then eluted with acetonitrile tetrahydrofuran. The eluent was analyzed with high-performance liquid chromatography. Findings showed more than 90% volatiles could be detected in the established method; the lowest determination limit was 0.0297 mg/mL; and the lowest quantification limit was 0.0991 mg/mL, which meant sensitivity and capability of the method were high. Regression coefficients of linear models between volatile concentrations and chromatographic peak characteristics were >0.995, indicating that the method could effectively and efficiently determine the contents of volatiles in automotive textiles.
EN
A simple capillary electrophoresis (CE) method with ultraviolet (UV) detection was developed for the determination of hexachlorophene (HCP) in cosmetics. Separation conditions were obtained in 20 mM Na2B4O7, 10% MeOH (pH 9.20), with 25 kV applied voltage and UV detection at 208 nm. Under the selected conditions, electrophoretic analysis was completed in about 4 min, with limit of detection (LOD) of 0.06 mg$mL1 for HCP. The method was successfully applied to determine HCP in three kinds of cosmetics with relative standard deviations (RSD) of 0.52–3.02% and recoveries from 90.0 to 96.4% for the spiked samples. The results indicated that the proposed method was reliable. Comparative experiments were also carried out with high-performance liquid chromatography (HPLC)-UV method described in National Standards of People’s Republic of China. The validation results of the two methods are comparable, but the proposed CE method is simple, rapid, which makes separation and analyte quantification in shorter time with much less reagent consumption.
6
Content available Metody oznaczania barwników spożywczych
EN
Food dyes are chemical substances that were developed to enhance the appearance of food by giving it artificial color. People have added colorings to food for centuries, but the first artificial food colorings were created in 1856 from coal tar. Over the years, hundreds of artificial food dyes have been developed, but a majority of them have since been found to be toxic. There is only a handful of artificial dyes that are still used in food. Food manufacturers often prefer artificial food dyes over natural food colorings, such as beta carotene and beet extract, because they produce a more vibrant color [1]. However, there is quite a bit of controversy regarding the safety of artificial food dyes. All of the artificial dyes that are currently used in food have gone through testing for toxicity in animal studies. Regulatory agencies, like the US Food and Drug Administration (FDA) and the European Food Safety Authority (EFSA), have concluded that the dyes do not pose significant health risks. Not everyone agrees with that conclusion. Interestingly, some food dyes are deemed safe in one country, but banned from human consumption in another, making it extremely confusing to assess their safety [2]. Undesirable effects of azo dyes used for coloring food products led to the development of very sensitive and selective analytical methods successfully used for their determination in various food matrices. Many different methods have been employed for the determination of synthetic dyes in food and beverages including thin layer chromatography and capillary electrophoresis [3]. However, these methods can be time consuming and may not be applicable for the simultaneous analysis of many dyes. Conventional HPLC methods have been employed for the analysis of synthetic colorants and while useful, these methods require long analysis times and large amounts of expensive solvents [4, 5]. Preparation of the test sample involves the use of various techniques such as membrane filtration due to the complexity of food products. Therefore, the development of simple, selective extraction methods together with the combination of chromatographic and spectrophotometric techniques are of great importance [6]. One of the most difficult stages of the analysis is the appropriate selection of the method for the determination of food colors. In the case of spectrophotometric methods, the main advantage is the low cost of the determination, however, the lack of specificity of the absorption spectrum usually makes it difficult to apply this method in the case of a mixture of different absorbing dyes due to the overlap of the spectra. The CE (Capillary Electrophoresis) analysis is faster and more economical compared to conventional electrophoresis and chromatography. The production of cheap capillaries and the development of on-line detection systems contributed to the development of modern capillary electrophoresis. Capillary electrophoresis has a number of types of separation. Ultimately, it is impossible to determine the one particular appropriate specific method for the determination of food dyes due to their diverse structure and chemical composition [4, 7].
EN
A novel, simple, robust, and rapid reversed-phased high-performance liquid chromatographic method has been developed for the separation and quantitative determination of the related substances of ezetimibe and simvastatin in combined dosage forms. Successful separation of the drug from the process-related impurities and degradation products formed under stress conditions was achieved on Inertsil ODS-3V (150 × 4.6 mm, 5.0 μm) column. The gradient liquid chromatography (LC) method employs solution A and solution B as mobile phase. The solution A contains 0.1% orthophosphoric acid solution in water, and solution B contains 0.1% orthophosphoric acid solution in acetonitrile. Flow rate was monitored at 2.0 mL/min, and the ultraviolet (UV) detection, at 238 nm. In forced degradation studies, the effect of acid, base, oxidation, UV light, and temperature was investigated, showing that good resolution between the peaks corresponds to process-related impurities and degradation products from both analyte. The performance of the method was validated according to the present International Conference on Harmonization (ICH) guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, ruggedness, and robustness. To the best of our knowledge, a rapid LC method, which separates all the impurities of ezetimibe and simvastatin in combined dosage forms, disclosed in this investigation was not published elsewhere.
EN
A reliable and rapid high-performance liquid chromatography coupled with diode array detector method (HPLC–DAD) was established and validated to determine eight gingerol simultaneously in the rhizomes of Zingiber offcinale Rosc. The separation of eight compounds (4-hydroxy-3-methoxy-benzenebutanol,3,5-dihydroxy-1-(4-hydroxy-3-methoxyphenyl) decane, 3,5-dihydroxy-1-(3,4-dimethoxyphenyl) decane, 6-gingerol, 8-gingerol, 6-shogaol, 5-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-1,4-decadien-3-one, and 10-gingerol) were performed on an Agilent TC(2) C18 (250 mm × 4.6 mm, 5 μm) at 30 °C using acetonitrile (A) and 1% formic acid aqueous solution (B) as the mobile phase with gradient elution (0–10 min, 20%–35% A; 10–28 min, 35%–55% A; 28–35 min, 55%–60% A; 35–55 min, 60%–70% A; 55.01–60 min, 100%–100% A). The detection wavelength was set at 280 nm, and the flow rate was 0.8 mL/min. Validation of the analytical method was performed by linearity, precision, and accuracy test. All compounds were quantified with good linear calibration curves (coefficient of determination R2, >0.9999). The method showed good precision with overall coefficients of variation between 0.56% and 0.84%. The range of recovery was from 95.50% to 104.14% for the analytes. This method was successfully applied to quantify eight gingerols in Z. offcinale Rosc from different regions in China, so it can provide quality assessment for this medicine.
EN
A newly proposed method for detecting content of adriamycin in pectin–adriamycin conjugate has been developed and evaluated. The content of adriamycin was detected by selective degradation of adramycin to adriamycinone. It was realized by a two-phase reaction system (water–chloroform reaction system), in which adriamycin was quantitatively converted to adriamycinone. Therefore, the latter can be used to calculate the precise content of adramycin in the polymer drug. To develop the method, the catalyst for degradation, the extraction solvent for adriamycinone, the temperature and time of degradation, and the ratio of pectin–adriamycin conjugate were investigated. The optimal reaction condition was as follows: 30 mg of pectin–adriamycin conjugate dissolved in 25 mL of water was added to a mixture of 25 mL of hydrochloric acid (1.5 mol/L) and 50 mL of chloroform; the mixture was heated to 40 °C to react for 1.5 h; after that, the mixture was extracted with chloroform for three times, and then the organic layer was combined and, subsequently, evaporated to remove solvent. Under this condition, adriamycinone generation rate reached 99.87%. The quantitative method was evaluated for linearity, the limit of detection (LOD) and limit of quantitation (LOQ), recovery, accuracy, robustness, and precision. The recoveries were between 99.47% and 101.07% with relative standard deviation <1.23%. The LOD and LOQ were 0.06 and 0.17 μg/mL, respectively. Compared to the traditional ultraviolet (UV) detection, this method is considered to be more precise for detecting content of adriamycin in its polymer conjugate.
EN
10-Methoxycamptothecin (MCPT) and 10-hydroxycamptothecin (HCPT) are the indole alkaloids isolated from a Chinese tree, Camptotheca acuminata, and have a wide spectrum of anticancer activity in vitro and in vivo mainly through inhibitory effects on topoisomerase I. HCPT is a major metabolite of MCPT in rats; the pharmacokinetic analysis and tissue distribution of MCPT and HCPT in rats have also been determined after i.v. injection of MCPT, but the excretion of MCPT and its metabolite HCPT has not been assessed up to now. In the present study, the excretion study of MCPT and its metabolite HCPT in rat bile, feces, and urine after i.v. administration of MCPT (5 mg kg-1) was performed by high performance liquid chromatography (HPLC) method coupled with a fluorescence detector. The results showed that MCPT mainly biotransformed to HCPT and excreted in the form of HCPT and MCPT in bile, urine, and feces after i.v. administration of MCPT. It was excreted about 1.24 ± 0.07% as MCPT and 5.49 ± 0.40% as HCPT in bile within 6 h after i.v. administration. The cumulative excretions of MCPT and HCPT were mainly within 24 h after i.v. administration, which were 0.41 ± 0.10% and 7.66 ± 1.43% of the dosage in urine and about 0.16 ± 0.04% and 20.30 ± 3.35% of the dosage in feces. The total excretion of MCPT in urine, bile, and feces was 1.81 ± 0.09% in the form of original MCPT and 33.45 ± 1.57%. detected as the metabolite HCPT in urine, bile, and feces, suggesting that MCPT might undergo other biotransformation.
PL
W artykule, na przykładzie kilku substancji czynnych farmaceutycznie, omówiono wpływ etapu przygotowania próbki na uzyskiwane wyniki analityczne podczas analizy HPLC. Przedstawiono wpływ rozpuszczalnika zastosowanego do rozpuszczania próbki badanej na stabilność roztworu, uzyskiwane parametry chromatograficzne oraz liniowość i czułość metody chromatograficznej. Omówiono również przykłady dotyczące przygotowania do analizy próbek substancji wykazujących fotolabilność w roztworze.
EN
In the article, the importance of the sample preparation step and its influence on analytical results have been demonstrated based on the investigations performed for selected active pharmaceutical ingredients. The impact of the solvent used for sample dissolution on the stability of solution, obtained chromatographic parameters, as well as the linearity and sensitivity of the chromatographic method has been presented. The examples of sample preparation for selected photolabile substances have been also included.
EN
A new and simple method based on high-performance liquid chromatography with ultraviolet detection (HPLC-UV) for the determination of cysteine (Cys) and cysteinylglycine (CysGly) in plasma and urine has been developed. The method involves reduction of disulfide bonds with tris(2-carboxyethyl)phosphine, derivatization of the analytes with 2-chloro-1-methylquinolinium tetrafluoroborate, and separation on Aeris PEPTIDE XB-C18 column (150 mm × 4.6 mm, 3.6 μm, Phenomenex) with UV detection at 355 nm. The calibration lines, obtained with human plasma and urine spiked with Cys- Gly and Cys, were linear in the range of 2.5–50 μmol L−1 and 20–300 μmol L−1, respectively. The intra- and inter-day precision values of the method, expressed as a relative standard deviation, were 0.25–11.1% and 0.71–12.3%, respectively. The analytical recovery varied from 89.7 to 112.3%. The LOQs for total Cys and CysGly were 1.5 pmol and 2.3 pmol in peak, respectively. The method was successfully applied to samples donated by apparently healthy individuals. Concentrations of Cys and CysGly in human plasma from 18 subjects varied from 141.6 to 217.8 μmol L−1 and from 21.1 to 50.9 μmol L−1, respectively. Their concentrations in urine samples (n = 14) ranged from 137.3 to 426.8 μmol L−1 and from 1.6 to 4.9 μmol L−1, respectively.
EN
Acetyl salicylic acid (ASA), as the major drug consumed in the world, has been combined with other various drugs. In this regard, ASA-rosuvastatin is the most recent combination. The current article reported the first two separation methods for the assay of that combination utilizing sequential injection chromatography (SIC) and high-performance liquid chromatography (HPLC). The optimization process was conducted for SIC, and the optimum conditions were then adapted to HPLC. Both methods, SIC and HPLC, were validated and successfully applied to tablet formulation. In both methods, the analytes were chromatographed onto a short C18 monolithic column (4.6 × 25 mm) by a mobile phase composition of 10 mmol L -1 phosphate:acetonitrile: methanol (50:30:20, v/v/v at pH 3.0). The performances of both methods were compared. The remarkable advantages of the SIC method over HPLC method were the reduction in reagent consumption and instrumentation simplicity and cost-effectiveness. The total volume of mobile phase consumed is three orders of magnitude larger in HPLC than that in SIC. Other analytical features of the SIC and HPLC methods were comparable and acceptable for pharmaceutical analysis. Accordingly, the SIC method could be more suitable for routine analysis of simple matrices after examining the capability of the technique to work under industrial conditions.
EN
A rapid high-performance liquid chromatography (HPLC) method for chiral purity determination of tenofovir disoproxil fumarate in raw material and pharmaceutical formulations was developed. The (S)-enantiomer appears to be as an impurity and pharmacologically inactive. The effects of various stationary phases, mobile phase composition, and column temperature on enantiomeric separation of tenofovir disoproxil were investigated and optimized. Chromatography resolution of tenofovir disoproxil enantiomers was performed on NUCLEOCEL ALPHA-RP S column (250 × 4.6 mm i.d., 5 μm). The elution was achieved by using 95:5% (υ/υ) methanol—acetonitrile, containing 0.1% triethylamine at a flow rate of 0.8 mL min−1. The ultraviolet (UV) detector was set at 260 nm. Calibration curves were linear in the range of 1–100 μg mL−1 and 0.2–20 μg mL−1 for (R)-tenofovir disoproxil and (S)-enantiomer, respectively. Limits of detection and quantitation for (S)-enantiomer were 0.06 and 0.2 μg mL−1. The run time of analysis was less than 7.0 min. The proposed method was used successfully for separation and quantification of tenofovir disoproxil enantiomers in raw material and pharmaceutical formulations.
EN
Andrographolide and betulinic acid are the terpenoids having potential anti-cancer activity. The cytotoxicity activity of both the drugs was carried out separately and in combination on liver cancer HepG2 cell lines. High-performance liquid chromatography (HPLC) and high-performance thin-layer chromatography (HPTLC) methods were developed and validated for simultaneous estimation of these two terpenoids as per the International Conference on Harmonization (ICH) guidelines, which was applied for quantification in nanoformulation. The retention time by HPLC and retardation factor by HPTLC for andrographolide and betulinic acid were found to be 2.2 and 6.6 min, and 0.24 ± 0.01 and 0.66 ± 0.01, respectively. Both the methods were validated for accuracy, precision, repeatability, robustness, limit of detection (LOD), and limit of quantitation (LOQ). The content of andrographolide and betulinic acid in nanoformulation was found to be 96.0% and 98.0% by HPLC and 96.59% and 98.33% by HPTLC, respectively, of labelled claim.
EN
Alcoholic-assisted dispersive liquid-liquid microextraction method (AADLLME) is used for the extraction, purification, and determination of bisphenol A in water samples by HPLC-UV. 1-octanol and methanol were selected as extraction and dispersive solvents of AA-DLLME procedure. The effects of several parameters of the AADLLME procedure (such as volume of extraction and dispersive solvents, amount of salt in sample solution, and extraction time) were investigated by a full factorial design. Then, the levels of significant factors were optimized using a central composite facecentered. The optimum conditions were obtained at 158 μL of extraction solvent, 500 μL of dispersive solvent, 1 min extraction time, and addition of 22% (w/v) of NaCl to the sample solution. Under optimum condition, the extraction recovery and the enrichment factor were determined, which were 91% and 65%, respectively. At these conditions, the limit of detection and the linearity were 0.10 and 1–100 μg L-1, respectively. The relative standard deviations for intra- and inter-day of extraction of bisphenol A (BPA) were 6.98% and 9.80%, respectively (for five measurements). Finally, the method was successfully applied for the determination of BPA in environmental water samples. In conclusion, it can be stated that the applied method is fast, simple, and environmentally friendly.
PL
Przedstawiona praca jest ostatnim projektem naukowym nad jakim pracował Profesor Henryk Lamparczyk, który przedwcześnie zmarł 16 listopada 2012 roku w wieku 65 lat. Przeglądowa praca o charakterze dydaktyczno-poglądowym dotyczy zastosowania cyklodekstryn w bioanalityce i została napisana w oparciu o prace opublikowane przez Profesora i współpracowników. Niniejsza wersja bazuje na artykule pt. “Natural cyclodextrins: development in theory, chromatography and pharmacy, A. Chmielewska, H. Lamparczyk;” opublikowanej w materiałach Supramolecular Chemistry and Advanced Materials. Wojciech Macyk & Konrad Szaciłowski, Editors, Kraków Jagielonian University 2007, pages 131-136 i jest rozszerzona o wiadomości przedstawione w najnowszych publikacjach dotyczących zastosowania cyklodekstryn w HPLC, głównie do oznaczeń sterydów i analiz przesiewowych próbek środowiskowych.
EN
This is the last research project of Professor Henryk Lamparczyk that prematurely passed away at age 65. In his intention it was to prepare a demonstrative review paper concerning application of cyclodextrins in bioanalysis, based on his and co-worker contributions to the field of supramolecular chemistry. This version of paper is based on the manuscript entitled “Natural cyclodextrins: development in theory, chromatography and pharmacy, A. Chmielewska, H. Lamparczyk;” that was published in Supramolecular Chemistry and Advanced Materials. Wojciech Macyk & Konrad Szaciłowski, Editors, Kraków Jagielonian University 2007, pages 131-136 and now is extended for the latest papers concerning HPLC application of cyclodextrins for steroids analysis and environmental samples screening. The main tools applied in described investigations were various chromatographic techniques such as gas chromatography (GC), high performance liquid chromatography (HPLC) and thin-layer chromatography (TLC). Topics such as structure-retention relationships, equilibrium constants between cyclodextrins (CDs) and guest molecules, thermodynamics and CDs separations were discussed. Additionally few examples of practical applications of CDs in pharmacy as well as biomedical and environmental analysis are given.
EN
A high-performance liquid chromatography (HPLC) method has been developed for simultaneous determination of six alkaloids, i.e., (−)-(R)-platydesmin, noroxyhydrastinine, berberine, skimmianine, canthin-6-one, and pteleine in the herbal medicine of Phellodendron amurense Rupr. The optimal condition for extraction and separation was achieved with a linear mobile phase gradient prepared from 0.1% phosphoric acid and acetonitrile. The LODs and LOQs for the analytes ranged from 0.06 to 0.22 μg mL-1 and from 0.25 to 0.80 μg mL-1, respectively. The optimized method was applied to the determination of alkaloids in P. amurense Rupr. and was found to be efficient. This method can provide a scientific and technical platform to the manufacturers for setting up a quality control standard as well as to the public for quality and safety assurance of the proprietary traditional Chinese medicines.
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